JP7308973B2 - Method for producing silicon carbide-silicon nitride composite material and silicon carbide-silicon nitride composite material thereby - Google Patents

Method for producing silicon carbide-silicon nitride composite material and silicon carbide-silicon nitride composite material thereby Download PDF

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JP7308973B2
JP7308973B2 JP2021561698A JP2021561698A JP7308973B2 JP 7308973 B2 JP7308973 B2 JP 7308973B2 JP 2021561698 A JP2021561698 A JP 2021561698A JP 2021561698 A JP2021561698 A JP 2021561698A JP 7308973 B2 JP7308973 B2 JP 7308973B2
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トカイ カーボン コリア カンパニー，リミティド
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Description

本発明は、炭化ケイ素－窒化ケイ素（ＳｉＣ－Ｓｉ３Ｎ４）複合材料の製造方法及びそれによる炭化ケイ素－窒化ケイ素（ＳｉＣ－Ｓｉ３Ｎ４）複合材料に関する。 The present invention relates to a method of manufacturing a silicon carbide-silicon nitride (SiC-Si 3 N 4 ) composite material and a silicon carbide-silicon nitride (SiC-Si 3 N 4 ) composite material thereby.

ＳｉＣ（炭化ケイ素）は、六方晶系の結晶構造を有する高温型（α型）、及び立方晶系の結晶構造を有する低温型（β型）が知られている。ＳｉＣは、Ｓｉに比べて耐熱性が高いだけではなく、広いバンドギャップを有し、絶縁破壊の電界強度が大きいという特徴がある。そのために、ＳｉＣ単結晶からなる半導体は、Ｓｉ半導体に代って次世代パワーデバイスの候補材料として期待されている。特に、α型ＳｉＣは、シリコンよりもバンドギャップが広いため、超低電力の損失パワーデバイスの半導体材料として注目を浴びている。 SiC (silicon carbide) is known as a high-temperature type (α-type) having a hexagonal crystal structure and a low-temperature type (β-type) having a cubic crystal structure. SiC not only has higher heat resistance than Si, but also has a wide bandgap and a large electric field strength for dielectric breakdown. Therefore, semiconductors made of SiC single crystals are expected as candidate materials for next-generation power devices in place of Si semiconductors. In particular, α-type SiC is attracting attention as a semiconductor material for ultra-low power loss power devices because it has a wider bandgap than silicon.

最近、ウェハーに直接的な影響を及ぼす半導体製造用部品素材に対する関心が増大しており、既存のＳｉｎｔｅｒｅｄ－ＳｉＣ素材よりも高温で耐変形性の高い清浄性及び化学的に耐食性に優れるＣＶＤ－ＳｉＣ素材を用いてプラズマガス制御装置が製造されれば、既存の素材に比べてプラズマガス制御装置の寿命が２～３倍増加するものと予測される。 Recently, there has been an increasing interest in materials for semiconductor manufacturing parts that directly affect wafers. If the material is used to manufacture a plasma gas control device, it is expected that the lifetime of the plasma gas control device will increase two to three times compared to existing materials.

ＣＶＤ－ＳｉＣ素材は、ＣＶＤ（化学的気相蒸着法）を用いてグラファイトにＳｉＣを積層させた後、グラファイトを取り除いた高純度のＳｉＣであり、このように作られたＣＶＤ－ＳｉＣは、表面平坦度のために研削加工を経てからプラズマガス制御装置の形状に応じる研削加工が行われる。 The CVD-SiC material is high-purity SiC obtained by stacking SiC on graphite using CVD (chemical vapor deposition) and then removing the graphite. After grinding for flatness, grinding according to the shape of the plasma gas control device is performed.

このようなＣＶＤ－ＳｉＣ素材で従来に幅広く使用されていたウェハーはダミーウェハー（ｄｕｍｍｙ ｗａｆｅｒ）であって、生産工程の初期に安全性を高めるために使用され、大きさ及び厚さが重要な要素として作用する。しかし、前記ダミーウェハーは、熱衝撃強度が４５０℃程度であり、工程時間を短縮するために急激な昇温及び冷却時に任意にクラックが生じ、Ｓｉウェハーの破損及び拡散（ｄｉｆｆｕｓｉｏｎ）装備の破損が現れた。 Wafers widely used in the past with such CVD-SiC materials are dummy wafers, which are used to improve safety in the early stage of the production process, and the size and thickness are important factors. acts as However, the dummy wafer has a thermal shock strength of about 450° C., and in order to shorten the process time, cracks are arbitrarily generated during rapid heating and cooling, which may damage the Si wafer and the diffusion equipment. Appeared.

従って、高純度及び高い熱衝撃強度を有する素材が求められている実状であり、単にシリコンカーバイトだけでなく、シリコンナイトライドのようなシリコン窒化物を混合した複合材に対する要求が高まっている。 Accordingly, materials having high purity and high thermal shock strength are in demand, and there is an increasing demand for composite materials containing not only silicon carbide but also silicon nitride such as silicon nitride.

特に、シリコン窒化物及びシリコンカーバイト複合材の高密度化、緻密性の確保などが改善されて機械的物性を改善させるための方法が研究されている。 In particular, methods for increasing the density of silicon nitride and silicon carbide composites, securing compactness, and improving mechanical properties are being investigated.

本発明は上述した問題を解決するためのもので、本発明の目的は 、鋳型を準備するステップ、及び前記鋳型上に１１００℃～１６００℃でＳｉ、Ｎ、及びＣを含む原料ガスを導入してＳｉＣ－Ｓｉ３Ｎ４複合材料を形成するステップを含むＳｉＣ－Ｓｉ３Ｎ４複合材料の製造方法を提供することにある。 An object of the present invention is to solve the above-mentioned problems. It is another object of the present invention to provide a method of manufacturing a SiC--Si 3 N 4 composite material, comprising the step of forming the SiC--Si 3 N 4 composite material.

しかし、本発明が解決しようとする課題は、以上で言及したものなどに制限されず、言及されない他の課題は下記の記載によって当該分野の当業者に明確に理解できるものである。 However, the problems to be solved by the present invention are not limited to those mentioned above, and other problems not mentioned will be clearly understood by those skilled in the art from the following description.

本発明の一実施形態に係るＳｉＣ－Ｓｉ３Ｎ４複合材料の製造方法は、鋳型を準備するステップと、前記鋳型上に１１００℃～１６００℃で、Ｓｉ、Ｎ、及びＣを含む原料ガスを導入してＳｉＣ－Ｓｉ３Ｎ４複合材料を形成するステップとを含む。 A method for producing a SiC-Si 3 N 4 composite material according to one embodiment of the present invention comprises the steps of preparing a mold, and applying a raw material gas containing Si, N, and C on the mold at 1100°C to 1600°C. introducing to form a SiC—Si 3 N 4 composite.

本発明の一実施形態により、前記導入する原料ガスのうち、窒素（Ｎ）と炭素（Ｃ）原料ガスの窒素（Ｎ）成分と炭素（Ｃ）成分が１：１である場合、Ｎソース／Ｃソースの比率が０．４～２であってもよい。 According to an embodiment of the present invention, when the nitrogen (N) component and the carbon (C) component of the nitrogen (N) and carbon (C) source gases among the introduced source gases are 1:1, N source/ The ratio of C source may be 0.4-2.

本発明の一実施形態により、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料のうち前記Ｓｉ３Ｎ４は、１０体積％～７０体積％であってもよい。 According to one embodiment of the present invention, the Si 3 N 4 in the SiC-Si 3 N 4 composite material may be 10 vol % to 70 vol %.

本発明の一実施形態により、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料の熱衝撃強度は、５００℃～８６０℃であってもよい。 According to one embodiment of the present invention, the thermal shock strength of said SiC-Si 3 N 4 composite may be between 500°C and 860°C.

本発明の一実施形態により、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料の熱衝撃強度は、６００℃～８６０℃であり、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料のうち前記Ｓｉ３Ｎ４は、４０体積％～７０体積％であってもよい。 According to one embodiment of the present invention, the SiC-Si 3 N 4 composite material has a thermal shock strength of 600° C. to 860° C., and the Si 3 N 4 in the SiC-Si 3 N 4 composite material is 40 It may be from vol % to 70 vol %.

本発明の一実施形態により、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料を形成するステップはＣＶＤ法に基づいてもよい。 According to one embodiment of the present invention, forming the SiC-Si 3 N 4 composite may be based on a CVD method.

本発明の他の一実施形態に係るＳｉＣ－Ｓｉ３Ｎ４複合材料は、ＳｉＣ及びＳｉ３Ｎ４を含み、熱衝撃強度が６００℃～８６０℃であってもよい。 A SiC-Si 3 N 4 composite according to another embodiment of the present invention may contain SiC and Si 3 N 4 and have a thermal shock strength of 600°C to 860°C.

本発明の一実施形態により、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料のうち前記Ｓｉ３Ｎ４は、１０体積％～７０体積％であってもよい。 According to one embodiment of the present invention, the Si 3 N 4 in the SiC-Si 3 N 4 composite material may be 10 vol % to 70 vol %.

本発明の一実施形態により、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料は、不定形のＳｉＣ結晶粒と針状構造のＳｉ３Ｎ４結晶粒が混合されていてもよい。 According to an embodiment of the present invention, the SiC-Si 3 N 4 composite material may be a mixture of amorphous SiC grains and acicular Si 3 N 4 grains.

本発明の一実施形態により、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料のうち、前記Ｓｉ３Ｎ４の体積比が６８体積％～７０体積％である場合、Ｓｉ３Ｎ４／ＳｉＣメインピークの回折強度比は０．２～１．５であってもよい。 According to one embodiment of the present invention, when the volume ratio of Si 3 N 4 in the SiC-Si 3 N 4 composite material is 68 vol % to 70 vol %, the Si 3 N 4 /SiC main peak diffraction The intensity ratio may be between 0.2 and 1.5.

本発明の一実施形態により、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料は、前述した一実施形態係る製造方法に基づいて製造されることができる。 According to an embodiment of the present invention, the SiC-Si 3 N 4 composite material can be manufactured according to the manufacturing method according to the embodiment described above.

本発明は、鋳型を準備するステップと、前記鋳型上に１１００℃～１６００℃でＳｉ、Ｎ、及びＣを含む原料ガスを導入してＳｉＣ－Ｓｉ３Ｎ４複合材料を形成するステップを含むＳｉＣ－Ｓｉ３Ｎ４複合材料の製造方法を提供することができる。
より詳細には、ＣＶＤ方式で熱衝撃強度が高い素材（Δ℃であるＳｉ３Ｎ４を共に成長させてＳｉＣ素材の熱衝撃強度を高め、半導体工程にも適用可能な高純度のＳｉＣ－Ｓｉ３Ｎ４複合材料を提供することができる。 The present invention comprises the steps of preparing a mold and introducing a source gas containing Si, N, and C onto the mold at 1100° C. to 1600° C. to form a SiC—Si 3 N 4 composite material. - A method for manufacturing Si3N4 composites can be provided.
In more detail, a material with high thermal shock strength (Si 3 N 4 with a temperature of Δ°C) is grown together with a CVD method to increase the thermal shock strength of the SiC material, and high-purity SiC-Si that can be applied to the semiconductor process. 3N4 composites can be provided.

従来におけるＳｉＣウェハー（ｄｕｍｍｙ ｗａｆｅｒ）の断面図である。1 is a cross-sectional view of a conventional SiC wafer (dummy wafer); FIG. 従来におけるＳｉＣウェハー（ｄｕｍｍｙ ｗａｆｅｒ）の表面微細構造のイメージである。1 is an image of a surface microstructure of a conventional SiC wafer (dummy wafer); 本発明の一実施形態により製造されたＳｉＣ－Ｓｉ３Ｎ４複合材料の表面微細構造のイメージである。4 is an image of the surface microstructure of a SiC-Si 3 N 4 composite fabricated according to one embodiment of the present invention; 本発明の一実施形態により製造されたＳｉＣ－Ｓｉ３Ｎ４複合材料のＮ／Ｃソース比によるＳｉ３Ｎ４含量比の変化グラフである。4 is a graph showing changes in Si 3 N 4 content ratio according to the N/C source ratio of a SiC-Si 3 N 4 composite material manufactured according to an embodiment of the present invention ; 本発明の一実施形態により製造されたＳｉＣ－Ｓｉ３Ｎ４複合材料のＮ／Ｃソース比によるＳｉ３Ｎ４の含量比が６９％であるとき、２－ｔｈｅｔａによる強度値グラフである。FIG. 5 is a graph of strength values according to 2-theta when the content ratio of Si 3 N 4 is 69% according to the N/C source ratio of the SiC—Si 3 N 4 composite material manufactured according to an embodiment of the present invention; FIG. 本発明の一実施形態により製造されたＳｉＣ－Ｓｉ３Ｎ４複合材料のＳｉ３Ｎ４含量による熱衝撃強度の変化を示したグラフである。4 is a graph showing changes in thermal shock strength according to Si 3 N 4 content of a SiC-Si 3 N 4 composite material manufactured according to an embodiment of the present invention;

以下、添付する図面を参照しながら本発明の実施形態を詳細に説明する。本発明の説明において、関連する公知機能又は構成に対する具体的な説明が本発明の要旨を不要に曖昧にすると判断される場合、その詳細な説明は省略する。また、本明細書で使用される用語は、本発明の好適な実施形態を適切に表現するために使用される用語であって、これはユーザ、運用者の意図又は本発明が属する分野の慣例などによって変わり得る。従って、本用語に対する定義は、本明細書全般にわたった内容に基づいて下されなければならないのであろう。各図面に提示されている同じ参照符号は同じ部材を示す。 Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. In the description of the present invention, if it is determined that a detailed description of related known functions or configurations unnecessarily obscures the gist of the present invention, the detailed description will be omitted. Also, the terms used in this specification are terms used to adequately express the preferred embodiments of the present invention, and may not reflect the intentions of the user, the operator, or the conventions of the field to which the present invention belongs. etc., can change. Therefore, the definition of this term should be made based on the general contents of this specification. The same reference numerals appearing in each drawing refer to the same parts.

明細書の全体において、いずれかの部材が他の部材「上に」位置しているとするとき、これはいずれかの部材が他の部材に接している場合だけでなく、２つの部材間に更なる部材が存在する場合も含み、詳細には、構成要素（ｅｌｅｍｅｎｔ）又は層が異なる要素又は層「上（ｏｎ）」、「に接続された（ｃｏｎｎｅｃｔｅｄ ｔｏ）」、又は「に結合された（ｃｏｕｐｌｅｄ ｔｏ）」ものとして示すとき、これが直接的に他の構成要素又は層にあるか、接続されるか、又は干渉構成要素又は層（ｉｎｔｅｒｖｅｎｉｎｇ ｅｌｅｍｅｎｔｓ ａｎｄ ｌａｙｅｒ）が存在し得ると理解される。 Throughout the specification, when any member is said to be "on" another member, this includes not only when the member is in contact with the other member, but also when the member is between the two members. In particular, an element or layer "on", "connected to" or "coupled to" a different element or layer, including when there are additional members. When indicated as "coupled to", it is understood that this may be directly in or connected to another element or layer, or there may be intervening elements and layers.

明細書全体において、ある部分がある構成要素を「含む」とするとき、これは、他の構成要素を取り除くものではなく、他の構成要素をさらに含むことを意味し、「含む」又は「有する」などの用語は、明細書上に記載された特徴、数字、段階、動作、構成要素、部品又はこれらを組み合わせたものが存在することを指定しようとするものであり、１つ又はそれ以上の異なる特徴や数字、段階、動作、構成要素、部品又はこれらを組み合わせたもの存在又は付加可能性を予め排除しないものと理解すべきである。 Throughout the specification, when a part "includes" a component, it means further including other components, not to the exclusion of other components. are intended to indicate the presence of any feature, figure, step, act, component, part, or combination thereof described in the specification, one or more It should be understood that the possibility of the presence or addition of different features, figures, steps, acts, components, parts or combinations thereof is not precluded.

異なるように定義さがれない限り、技術的であるか又は科学的な用語を含むここで用いる全ての用語は、本実施形態が属する技術分野で通常の知識を有する者によって一般的に理解されるものと同じ意味を有する。一般的に用いられる予め定義された用語は、関連技術の文脈上で有する意味と一致する意味を有するものと解釈すべきであって、本明細書で明白に定義しない限り、理想的又は過度に形式的な意味として解釈されることはない。 Unless defined otherwise, all terms, including technical or scientific terms, used herein are commonly understood by one of ordinary skill in the art to which the embodiments belong. have the same meaning as Commonly used pre-defined terms are to be construed to have a meaning consistent with the meaning they have in the context of the relevant art, and unless expressly defined herein, are ideally or excessively It is not to be interpreted in a formal sense.

また、図面を参照して説明する際に、図面符号に拘わらず同じ構成要素は同じ参照符号を付与し、これに対する重複する説明は省略する。実施形態の説明において関連する公知技術に対する具体的な説明が本発明の要旨を不要に曖昧にすると判断される場合、その詳細な説明は省略する。 In addition, when describing with reference to the drawings, the same constituent elements will be given the same reference numerals regardless of the drawing numerals, and redundant description thereof will be omitted. In the description of the embodiments, when it is determined that a detailed description of related known technology unnecessarily obscures the gist of the present invention, the detailed description will be omitted.

以下、本発明のＳｉＣ－Ｓｉ３Ｎ４複合材料の製造方法及びこれによって製造されたＳｉＣ－Ｓｉ３Ｎ４複合材料について、実施形態及び図面を参照して具体的に説明する。しかし、本発明がこのような実施形態及び図面に制限されることはない。
以下、実施形態及び比較例により本発明をより詳細に説明する。 Hereinafter, the method for producing a SiC-Si 3 N 4 composite material of the present invention and the SiC-Si 3 N 4 composite material produced by the method will be specifically described with reference to embodiments and drawings. However, the invention is not limited to such embodiments and drawings.
BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in more detail with reference to embodiments and comparative examples.

但し、下記の実施形態は、本発明を例示するためのものに過ぎず、本発明の内容が下記の実施形態により限定されることはない。 However, the following embodiments are merely for illustrating the present invention, and the content of the present invention is not limited by the following embodiments.

本発明の一実施形態に係るＳｉＣ－Ｓｉ３Ｎ４複合材料の製造方法は、鋳型を準備するステップ、及び前記鋳型上に１１００℃～１６００℃でＳｉ、Ｎ、及びＣを含む原料ガスを導入してＳｉＣ－Ｓｉ３Ｎ４複合材料を形成するステップを含む。 A method for producing a SiC-Si 3 N 4 composite material according to an embodiment of the present invention comprises the steps of preparing a mold, and introducing a raw material gas containing Si, N, and C at 1100° C. to 1600° C. onto the mold. to form a SiC-Si 3 N 4 composite.

一側面によると、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料は、ＳｉＣに比べて相対的に高い熱衝撃強度を有するＳｉ３Ｎ４素材を含んでもよい。 According to one aspect, the SiC-Si 3 N 4 composite material may include a Si 3 N 4 material having relatively high thermal shock strength compared to SiC.

一側面によると、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料は、ＣＶＤ方式に基づいて製造し、半導体工程のうち拡散工程のような５００℃以上の熱衝撃強度が求められる製品群に適用してもよい。 According to one aspect, the SiC-Si 3 N 4 composite material is manufactured based on a CVD method, and can be applied to a group of products requiring thermal shock strength of 500° C. or higher, such as a diffusion process among semiconductor processes. good.

一側面によると、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料のＳｉＣ－Ｓｉ３Ｎ４は、５００℃以上の熱衝撃を繰り返して加えられる過酷な工程で使用可能なもので、熱衝撃強度（ΔＴ）が１０００℃又はそれ以上であってもよい。 According to one aspect, the SiC-Si 3 N 4 of the SiC-Si 3 N 4 composite material can be used in a severe process in which thermal shocks of 500 ° C. or higher are repeatedly applied, and has a thermal shock strength (ΔT) of may be 1000° C. or higher.

一側面によると、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料を製造するためには、ＣＶＤ法に基づいて製造されることが好ましい。 According to one aspect, the SiC--Si 3 N 4 composite material is preferably manufactured based on a CVD method.

一側面によると、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料は、強度、非弾性が高く、優れた高温強度及び熱衝撃に強い性質を有し、それだけでなく、高温酸化雰囲気で酸化問題も改善されたものである。 According to one aspect, the SiC-Si 3 N 4 composite material has high strength, high inelasticity, excellent high-temperature strength and thermal shock resistance properties, as well as improved oxidation problem in high-temperature oxidizing atmosphere. It is a thing.

一側面によると、前記ＳｉＣは融点が高く、靭性が良くて耐酸化性及び耐摩耗性に優秀なものであれば、特に制限されることはない。 According to one aspect, SiC is not particularly limited as long as it has a high melting point, good toughness, and excellent oxidation resistance and wear resistance.

一側面によると、前記Ｓｉ３Ｎ４は内部に酸素が存在せず、酸素の拡散係数が極めて低い材料であって、酸素に対するバリア（ｂａｒｒｉｅｒ）の役割を果たして高温における破壊強度、破壊靱性、耐熱衝撃特性に優れ、特に、耐摩耗性の側面でＳｉＣよりも優れる。 According to one aspect, the Si 3 N 4 is a material that does not contain oxygen and has a very low diffusion coefficient of oxygen. It has excellent impact properties, and is superior to SiC in terms of wear resistance.

一側面によると、前記鋳型を準備するステップにおいて、前記鋳型はＳｉＣを含んでもよく、前記ＳｉＣを含む鋳型は、焼結法又はＣＶＤを用いて製造されたものであってもよい。当技術分野で幅広く知られたＳｉＣ焼結方法又はＳｉＣ ＣＶＤ（化学気相蒸着法）であれば、制限されることなく使用されてＳｉＣ素材の鋳型を準備することができる。 According to one aspect, in the step of preparing the mold, the mold may contain SiC, and the mold containing SiC may be manufactured using a sintering method or CVD. Any SiC sintering method or SiC CVD (Chemical Vapor Deposition), which is widely known in the art, can be used without limitation to prepare the SiC material mold.

一側面によると、前記鋳型上に１１００℃～１６００℃であり、Ｓｉ、Ｎ、及びＣを含む原料ガスを導入してＳｉＣ－Ｓｉ３Ｎ４複合材料を形成するステップにおいて、前記原料ガスの供給の速度又は種類に応じて、ＳｉＣ－Ｓｉ３Ｎ４複合材料の物性が変わり得る。 According to one aspect, in the step of forming a SiC—Si 3 N 4 composite material by introducing a source gas having a temperature of 1100° C. to 1600° C. and containing Si, N, and C onto the mold, the source gas is supplied. Depending on the rate or type of , the physical properties of the SiC-Si 3 N 4 composite can vary.

一側面によると、前記Ｓｉ、Ｎ、及びＣを含む原料ガスは、ケイ素、窒素、及び炭素を供給できるガスであれば特に制限されないが、その一例として、ＴＣＳ、ＭＴＳ、ＳＨ４、ＳｉＣｌ４、Ｎ２、ＨＮ３、ＣＨ４及びＣ３Ｈ８からなる群から選択される１つ以上を含んでもよい。 According to one aspect, the raw material gas containing Si, N, and C is not particularly limited as long as it is a gas capable of supplying silicon, nitrogen , and carbon. It may contain one or more selected from the group consisting of N2 , HN3 , CH4 and C3H8 .

一側面によると、前記Ｓｉ、Ｎ、及びＣを含む原料ガスは、ケイ素、窒素、及び炭素を全て含み、一種類のガス供給だけでＣＶＤによる蒸着が行われてもよく、ケイ素、窒素又は炭素をそれぞれ含む各原料ガスの複合的な供給により段階的にＣＶＤによる蒸着が行われてもよい。 According to one aspect, the source gas containing Si, N, and C contains all of silicon, nitrogen, and carbon, and deposition by CVD may be performed by supplying only one type of gas, such as silicon, nitrogen, or carbon. Deposition by CVD may be performed step by step by composite supply of each source gas respectively containing .

一側面によると、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料を形成するステップは様々な温度で実行されてもよいが、熱的ＣＶＤを使用する場合１１００℃～１６００℃で実行されることが好ましく、１１００℃よりも低い温度では蒸着が実行され難く、１６００℃よりも高温では蒸着し難いか、鋳型が損傷するという恐れがある。 According to one aspect, the step of forming said SiC-Si 3 N 4 composite may be performed at various temperatures, but is preferably performed between 1100° C. and 1600° C. when using thermal CVD; At temperatures lower than 1100° C., deposition is difficult to perform, and at temperatures higher than 1600° C., deposition is difficult or the mold may be damaged.

一側面によると、前記Ｓｉ、Ｎ、及びＣを含む原料ガスを導入してＳｉＣ－Ｓｉ３Ｎ４複合材料を形成するステップは、Ｓｉ、Ｎ、及びＣを含む原料ガスをＣＶＤ蒸着装置の反応チャンバ内に注入するステップを含んでもよく、前記反応チャンバ内に注入されるガスは、Ｓｉ、Ｎ、及びＣを含む原料ガスの他にも不活性ガスをさらに含んでもよい。 According to one aspect, the step of introducing the source gas including Si, N, and C to form the SiC—Si 3 N 4 composite material includes reacting the source gas including Si, N, and C in a CVD deposition apparatus. A step of injecting into a chamber may be included, and the gas injected into the reaction chamber may further include an inert gas in addition to source gases containing Si, N, and C.

一側面によると、前記反応チャンバ内の蒸着圧力は４００ｔｏｒｒ～７００ｔｏｒｒであってもよい。 According to one aspect, the deposition pressure in the reaction chamber may be between 400 torr and 700 torr.

本発明の一実施形態により、前記導入する原料ガスのうち、窒素（Ｎ）と炭素（Ｃ）原料ガスの窒素（Ｎ）成分と炭素（Ｃ）成分が１：１である場合、Ｎソース／Ｃソースの比率が０．４～２であってもよい。 According to an embodiment of the present invention, when the nitrogen (N) component and the carbon (C) component of the nitrogen (N) and carbon (C) source gases among the introduced source gases are 1:1, N source/ The ratio of C source may be 0.4-2.

一側面によると、前記数値範囲内のＮソース／Ｃソースの比率を有する原料ガスを導入する場合、ＳｉＣ及びＳｉ３Ｎ４の比率が適切に調和され、熱衝撃強度が高くて急激な昇温及び冷却時にもクラックが発生しない、優秀なＳｉＣ－Ｓｉ３Ｎ４複合材料を製造することができる。 According to one aspect, when a raw material gas having an N source/C source ratio within the numerical range is introduced, the ratio of SiC and Si 3 N 4 is properly balanced, and the thermal shock strength is high and the temperature rises rapidly. Also, an excellent SiC--Si 3 N 4 composite material, which does not generate cracks even when cooled, can be produced.

図４は、本発明の一実施形態により製造されたＳｉＣ－Ｓｉ３Ｎ４複合材料のＮソース／Ｃソース比によるＳｉ３Ｎ４の含量比の変化グラフである。図４に示すように、Ｎソース／Ｃソース比が０．４～２である場合、Ｓｉ３Ｎ４の含量比が約１０％～７０％になり、ＳｉＣ－Ｓｉ３Ｎ４複合材料内で一定の含量比を含み、優秀な熱衝撃強度を確保することができる。 FIG. 4 is a graph showing changes in the content ratio of Si 3 N 4 according to the N source/C source ratio of the SiC—Si 3 N 4 composite material manufactured according to an embodiment of the present invention. As shown in FIG. 4, when the N source/C source ratio is 0.4-2, the content ratio of Si 3 N 4 is about 10%-70%, and the SiC—Si 3 N 4 composite material It contains a certain content ratio and can ensure excellent thermal shock strength.

図５は、本発明の一実施形態により製造されたＳｉＣ－Ｓｉ３Ｎ４複合材料のＮソース／Ｃソース比＝２によるＳｉ３Ｎ４の含量比が６９％であれば、２－ｔｈｅｔａによる強度値グラフであって、β－ＳｉＣ及びα－Ｓｉ３Ｎ４結晶構造を意味し、Ｓｉ３Ｎ４の含量比により各 結晶構造のメインピークの回折強度比が変化することになる。図５に示すように、Ｓｉ３Ｎ４の含量比が６９％である場合には、Ｓｉ３Ｎ４メインピークの回折強度／ＳｉＣメインピークの回折強度比が１．５になる。 FIG. 5 shows the SiC-Si 3 N 4 composite material manufactured according to one embodiment of the present invention, where the N source/C source ratio = 2 and the Si 3 N 4 content ratio is 69%, according to 2-theta In the intensity value graph, it means β-SiC and α-Si 3 N 4 crystal structures, and the diffraction intensity ratio of the main peak of each crystal structure changes according to the content ratio of Si 3 N 4 . As shown in FIG. 5, when the content ratio of Si 3 N 4 is 69%, the ratio of diffraction intensity of Si 3 N 4 main peak/diffraction intensity of SiC main peak is 1.5.

本発明の一実施形態により、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料のうち前記Ｓｉ３Ｎ４は、１０体積％～７０体積％であってもよい。 According to one embodiment of the present invention, the Si 3 N 4 in the SiC-Si 3 N 4 composite material may be 10 vol % to 70 vol %.

一側面によると、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料のうち、Ｓｉ３Ｎ４の体積含量が１０体積％未満である複合材料であれば、Ｓｉ３Ｎ４の含量が小さ過ぎて熱衝撃強度が低く、急激な温度変化によりクラックが発生することで拡散装備が破損する一方、Ｓｉ３Ｎ４の体積含量が７０体積％超過すれば、Ｓｉ３Ｎ４の含量が高過ぎてＳｉＣの含量が低くなり、ＣＶＤ蒸着による成長が困難になる。 According to one aspect, among the SiC—Si 3 N 4 composite materials, if the Si 3 N 4 volume content is less than 10% by volume, the Si 3 N 4 content is too small, resulting in poor thermal impact strength. If the Si3N4 volume content exceeds 70% by volume, the Si3N4 content is too high and the SiC content is low . low and difficult to grow by CVD deposition.

本発明の一実施形態により、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料の熱衝撃強度は、５００℃～８６０℃であってもよい。 According to one embodiment of the present invention, the thermal shock strength of said SiC-Si 3 N 4 composite may be between 500°C and 860°C.

一側面によると、前記熱衝撃強度の測定は、ＫＳ Ｌ１６１１測定方法により測定してもよい。 According to one aspect, the thermal shock strength may be measured by KS L1611 measurement method.

一側面によると、前記熱衝撃強度は、急激な昇温及び冷却による温度差に基づいてもクラックが発生することなく耐える物性を意味し、ΔＴのように現してもよい。 According to one aspect, the thermal shock strength refers to a physical property that withstands a temperature difference due to rapid heating and cooling without cracking, and may be expressed as ΔT.

一側面によると、前記熱衝撃強度が５００℃～８６０℃であることは、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料が５００℃～８６０℃の温度差でもクラックが発生することなく、Ｓｉウェハーの破損及び拡散装備の破損が生じないことを意味する。 According to one aspect, the thermal shock strength of 500° C. to 860° C. means that the SiC—Si 3 N 4 composite material does not crack even when the temperature difference is 500° C. to 860° C., and the Si wafer breaks. and that no damage to the diffusion equipment will occur.

一側面によると、前記熱衝撃強度が５００℃未満であれば、半導体ウェハー工程において、反復的な熱衝撃により頻繁なクラックが発生する恐れがあり、８６０℃を超過すれば現実的な製造が難しい。 According to one aspect, if the thermal shock strength is less than 500° C., frequent cracks may occur due to repeated thermal shocks in the semiconductor wafer process, and if it exceeds 860° C., practical manufacturing is difficult. .

本発明の一実施形態により、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料の熱衝撃強度は、６００℃～８６０℃であり、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料のうち、前記Ｓｉ３Ｎ４は、４０体積％～７０体積％であってもよい。 According to one embodiment of the present invention, the SiC—Si 3 N 4 composite material has a thermal shock strength of 600° C. to 860° C. In the SiC—Si 3 N 4 composite material, the Si 3 N 4 is It may be 40% to 70% by volume.

一側面によると、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料の熱衝撃強度は、６００℃～８６０℃であることが好ましい。 According to one aspect, the SiC-Si 3 N 4 composite material preferably has a thermal shock strength of 600°C to 860°C.

一側面によると、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料のうち、熱衝撃強度を高めるために混合するＳｉ３Ｎ４の体積含量は、４０体積％～７０体積％であることが好ましい。 According to one aspect, the volume content of Si 3 N 4 mixed in the SiC-Si 3 N 4 composite material to increase thermal shock strength is preferably 40 vol % to 70 vol %.

図６は、本発明の一実施形態により製造されたＳｉＣ－Ｓｉ３Ｎ４複合材料のＳｉ３Ｎ４含量による熱衝撃強度の変化を示したグラフであり、Ｓｉ３Ｎ４含量が４０％を超過する時点で熱衝撃強度が６００℃以上であり、Ｓｉ３Ｎ４含量が８０％未満になるまで、熱衝撃強度が７００℃未満まで急速に増加することが確認される。 FIG. 6 is a graph showing changes in thermal shock strength according to Si 3 N 4 content of a SiC-Si 3 N 4 composite material manufactured according to an embodiment of the present invention, where the Si 3 N 4 content is 40%. It is confirmed that the thermal shock strength is 600° C. or higher at the point of excess, and the thermal shock strength rapidly increases to less than 700° C. until the Si 3 N 4 content is less than 80%.

本発明の一実施形態により、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料を形成するステップはＣＶＤ法に基づいてもよい。 According to one embodiment of the present invention, forming the SiC-Si 3 N 4 composite may be based on a CVD method.

一側面によると、前記ＣＶＤ法は通常使用されるＣＶＤ（化学気相蒸着法）であれば特に制限されず、その一例として、誘導結合プラズマ化学蒸着（Ｉｎｄｕｃｔｉｖｅｌｙ Ｃｏｕｐｌｅｄ Ｐｌａｓｍａ－ＣｈｅｍｉｃａｌＶａｐｏｒ Ｄｅｐｏｓｉｔｉｏｎ；ＩＣＰ－ＣＶＤ）、低圧化学蒸着（Ｌｏｗ Ｐｒｅｓｓｕｒｅ ＣｈｅｍｉｃａｌＶａｐｏｒ Ｄｅｐｏｓｉｔｉｏｎ；ＬＰＣＶＤ）、常圧化学蒸着（Ａｔｍｏｓｐｈｅｒｉｃ Ｐｒｅｓｓｕｒｅ ＣｈｅｍｉｃａｌＶａｐｏｒ Ｄｅｐｏｓｉｔｉｏｎ；ＡＰＣＶＤ）及びプラズマ化学蒸着（Ｐｌａｓｍａ－ｅｎｈａｎｃｅｄ ｃｈｅｍｉｃａｌ ｖａｐｏｒ ｄｅｐｏｓｉｔｉｏｎ；ＰＥＣＶＤ）が含まれてもよい。 According to one aspect, the CVD method is not particularly limited as long as it is a commonly used CVD (Chemical Vapor Deposition) method, and an example thereof is Inductively Coupled Plasma-Chemical Vapor Deposition (ICP-CVD). , Low Pressure Chemical Vapor Deposition (LPCVD), Atmospheric Pressure Chemical Vapor Deposition (APCVD) and Plasma-enhanced chemical vapor deposition. on; PECVD) may be included.

本発明の一実施形態により、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料は、不浸透性を有してもよい。 According to one embodiment of the present invention, said SiC-Si 3 N 4 composite may be impermeable.

一側面によると、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料は、従来におけるＳｉＣの透過特性を改善させて不透過特性を示し、高純度及び高い熱衝撃強度を有することができる。 According to one aspect, the SiC-Si 3 N 4 composite material can improve the permeation property of conventional SiC, exhibit non-permeation property, and have high purity and high thermal shock strength.

本発明の更なる一実施形態に係るＳｉＣ－Ｓｉ３Ｎ４複合材料は、ＳｉＣ及びＳｉ３Ｎ４を含み、熱衝撃強度が６００℃～８６０℃である。 A further embodiment of the present invention is a SiC-Si3N4 composite comprising SiC and Si 3 N 4 and having a thermal shock strength of 600°C to 860°C.

一側面によると、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料は、ＳｉＣ及びＳｉ３Ｎ４が混合したもので、６００℃～８６０℃の急激な温度差でもクラックが発生しない。 According to one aspect, the SiC-Si 3 N 4 composite material is a mixture of SiC and Si 3 N 4 , and does not crack even under a sudden temperature difference of 600°C to 860°C.

本発明の一実施形態により、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料のうち前記Ｓｉ３Ｎ４は、１０体積％～７０体積％であってもよい。 According to one embodiment of the present invention, the Si 3 N 4 in the SiC-Si 3 N 4 composite material may be 10 vol % to 70 vol %.

一側面によると、前記Ｓｉ３Ｎ４の体積比は、ＸＲＤ装備（Ｒｅｇａｋｕ、ＤＭＡＸ２０００）を用いて測定電圧と電流値がそれぞれ４０ｋＶ、４０ｍＡであり、ｓｃａｎ ｓｐｅｅｄ１０、ｓｃａｎ ｓｔｅｐ０．０５で測定し、測定されたデータ上でＪＣＰＤＳデータと同じβとα－Ｓｉ３Ｎ４のピークが全て現れ、各ＳｉＣとＳｉ３Ｎ４の結晶相のピーク面積に総和に対する比率に基づいて分析したものである。 According to one aspect, the Si 3 N 4 volume ratio was measured using an XRD device (Regaku, DMAX2000) at a voltage and current of 40 kV and 40 mA, respectively, at a scan speed of 10 and a scan step of 0.05. β and α-Si 3 N 4 peaks, which are the same as those in the JCPDS data, appear on the data obtained, and are analyzed based on the ratio to the sum of the peak areas of each SiC and Si 3 N 4 crystal phase.

一側面によると、前記ＳｉＣ－Ｓｉ３Ｎ４複合素材のうち前記Ｓｉ３Ｎ４は、４０体積％～７０体積％であることが好ましい。 According to one aspect, the Si 3 N 4 in the SiC-Si 3 N 4 composite material is preferably 40 vol % to 70 vol %.

本発明の一実施形態により、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料は、不定形のＳｉＣ結晶粒と針状構造のＳｉ３Ｎ４結晶粒が混合したものであってもよい。 According to an embodiment of the present invention, the SiC-Si 3 N 4 composite material may be a mixture of amorphous SiC grains and acicular Si 3 N 4 grains.

一側面によると、前記ＳｉＣ結晶粒は、不定形の薄い片状であってもよく、前記Ｓｉ３Ｎ４結晶粒は針状構造として互いに混合したものであってもよい。 According to one aspect, the SiC grains may be amorphous thin flakes, and the Si 3 N 4 grains may be mixed with each other as needle-like structures.

図２は、従来におけるＳｉＣウェハーの表面微細構造のイメージであり、図３は、本発明の一実施形態により製造されたＳｉＣ－Ｓｉ３Ｎ４複合材料の表面微細構造のイメージである。図２に示すように、従来におけるＳｉＣだけを用いたウェハーの場合、不定形の薄い片状の断面構造のみが示されていることが確認され、本発明の一実施形態により製造されたＳｉＣ－Ｓｉ３Ｎ４複合材料の場合、図３において、不定形のＳｉＣ結晶粒と針状構造のＳｉ３Ｎ４結晶粒とが混合していることが確実に確認される。 FIG. 2 is an image of the surface microstructure of a conventional SiC wafer, and FIG. 3 is an image of the surface microstructure of a SiC—Si 3 N 4 composite fabricated according to one embodiment of the present invention. As shown in FIG. 2, in the case of the conventional wafer using only SiC, it was confirmed that only an irregular thin flake cross-sectional structure was shown. In the case of the Si 3 N 4 composite material, it is definitely confirmed in FIG. 3 that amorphous SiC crystal grains and needle-like Si 3 N 4 crystal grains are mixed.

発明の一実施形態により、前記ＳｉＣ－Ｓｉ３Ｎ４複合素材のうち前記Ｓｉ３Ｎ４の体積比が６８体積％～７０体積％である場合、Ｓｉ３Ｎ４／Ｓｉ Ｃメインピークの回折強度比は０．２～１．５であってもよい。 According to an embodiment of the invention, when the volume ratio of Si3N4 in the SiC- Si3N4 composite material is 68 % to 70% by volume, the diffraction intensity of Si3N4 /SiC main peak The ratio may be between 0.2 and 1.5.

図４は、本発明の一実施形態により製造されたＳｉＣ－Ｓｉ３Ｎ４複合材料のＮソース／Ｃソース比によるＳｉ３Ｎ４の含量比の変化グラフである。図４に示すように、Ｎソース／Ｃソース比が０．４～２である場合、Ｓｉ３Ｎ４の含量比が約１０％～７０％になって、ＳｉＣ－Ｓｉ３Ｎ４複合材料内で一定の含量比を含み、優れる熱衝撃強度を確保することができる。 FIG. 4 is a graph showing changes in the content ratio of Si 3 N 4 according to the N source/C source ratio of the SiC—Si 3 N 4 composite material manufactured according to an embodiment of the present invention. As shown in FIG. 4, when the N source/C source ratio is 0.4 to 2, the content ratio of Si 3 N 4 is about 10% to 70%, and the SiC—Si 3 N 4 composite material contains contains a certain content ratio to ensure excellent thermal shock strength.

図５は、本発明の実施形態により製造されたＳｉＣ－Ｓｉ３Ｎ４複合素材のＮソース／Ｃソース比＝２によるＳｉ３Ｎ４の含量比が６９％であるとき、２－ｔｈｅｔａによる強度値グラフであって、β－ＳｉＣ及びα－Ｓｉ３Ｎ４結晶構造を意味し、Ｓｉ３Ｎ４の含量比により各 結晶構造のメインピークの回折強度比が変化する。図５に示すように、Ｓｉ３Ｎ４の含量比が６９％である場合、Ｓｉ３Ｎ４メインピークの回折強度／ＳｉＣメインピークの回折強度比が１．５になる。 FIG. 5 shows the intensity by 2-theta when the content ratio of Si 3 N 4 is 69% by N source/C source ratio=2 of the SiC-Si 3 N 4 composite material manufactured according to the embodiment of the present invention. It is a value graph, which means β-SiC and α-Si 3 N 4 crystal structures, and the diffraction intensity ratio of the main peak of each crystal structure changes according to the content ratio of Si 3 N 4 . As shown in FIG. 5, when the content ratio of Si 3 N 4 is 69%, the ratio of diffraction intensity of Si 3 N 4 main peak/diffraction intensity of SiC main peak is 1.5.

本発明の一実施形態により、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料は、不浸透性を有してもよい。 According to one embodiment of the present invention, said SiC-Si 3 N 4 composite may be impermeable.

一側面によると、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料は、従来におけるＳｉＣの透過特性を改善させて不透過特性を示し、高純度及び高い熱衝撃強度を有し得る。 According to one aspect, the SiC-Si 3 N 4 composite material can improve the permeable property of conventional SiC to exhibit non-permeable property, and have high purity and high thermal shock strength.

本発明の一実施形態により、前記ＳｉＣ－Ｓｉ３Ｎ４複合材料は、前述した一実施形態に係る製造方法に基づいて製造されることができる。 According to an embodiment of the present invention, the SiC-Si 3 N 4 composite material can be manufactured according to the manufacturing method according to the embodiment described above.

以下、実施形態及び比較例によって本発明をより詳細に説明する。 BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in more detail with reference to embodiments and comparative examples.

但し、下記の実施形態は本発明を例示するためのもので、本発明の内容が下記の実施形態に限定されることはない。 However, the following embodiments are intended to illustrate the present invention, and the content of the present invention is not limited to the following embodiments.

実施形態：ＳｉＣ－Ｓｉ ３ Ｎ ４ 複合材料の製造
ＣＶＤ方式に基づいてＳｉ３Ｎ４とＳｉＣが形成される温度である１１００℃～１６００℃においてＳｉ、Ｎ、Ｃソースを投入し、ＳｉＣ－Ｓｉ３Ｎ４複合素材を製造した。 Embodiment: Production of SiC-Si 3 N 4 composite material SiC-Si by adding Si, N, C sources at 1100 ° C to 1600 ° C, which is the temperature at which Si 3 N 4 and SiC are formed based on the CVD method. A 3N4 composite was fabricated.

この場合、Ｎソース／Ｃソース比は窒素（Ｎ）と炭素（Ｃ）原料ガスの窒素（Ｎ）成分と炭素（Ｃ）成分が１：１である場合にＮソース／Ｃソース比に関し、０．４～２であり、全体の素材でＳｉ３Ｎ４の体積比は１３％～７０％であった。 In this case, the N source/C source ratio is 0 with respect to the N source/C source ratio when the nitrogen (N) component and the carbon (C) component of the nitrogen (N) and carbon (C) source gas are 1:1. .4 to 2, and the volume ratio of Si 3 N 4 in the entire material was 13% to 70%.

このような複合材料ＳｉＣ－Ｓｉ３Ｎ４複合材料の熱衝撃強度は、熱衝撃強度測定器で測定した結果、Δ＝６００℃～８６０℃で測定された。 The thermal shock strength of such a composite material SiC--Si 3 N 4 composite material was measured at Δ=600° C. to 860° C. as a result of measuring with a thermal shock strength tester.

図１は、従来におけるＳｉＣウェハーの断面図であり、図２は、従来におけるＳｉＣウェハーの表面微細構造のイメージである。 FIG. 1 is a cross-sectional view of a conventional SiC wafer, and FIG. 2 is an image of the surface fine structure of the conventional SiC wafer.

図３は、一実施形態により製造されたＳｉＣ－Ｓｉ３Ｎ４複合材料の表面微細構造のイメージであって、図２と比較するとき、針状と不定形の結晶粒が混合したものが確認された。これによって従来の図２に基づいた不定形構造のＳｉＣウェハーと比較するとき、針状構造のＳｉ３Ｎ４が含まれていることが確かに確認された。 FIG. 3 is an image of the surface microstructure of a SiC—Si 3 N 4 composite fabricated according to one embodiment, showing a mixture of acicular and amorphous grains when compared to FIG. was done. Thus, it was confirmed that needle-shaped Si 3 N 4 was included when compared with the conventional SiC wafer with an amorphous structure based on FIG. 2 .

図４は、本発明の一実施形態により製造されたＳｉＣ－Ｓｉ３Ｎ４複合材料のＮソース／Ｃソース比によるＳｉ３Ｎ４の含量比の変化グラフであり、図４に示すように、Ｎソース／Ｃソース比が０．４～２である場合、Ｓｉ３Ｎ４の含量比が約１０％～７０％になり、ＳｉＣ－Ｓｉ３Ｎ４複合材料のうち一定の含量比を含み、優れる熱衝撃強度を確保できることが確認された。 FIG. 4 is a graph showing changes in the content ratio of Si 3 N 4 according to the N source/C source ratio of the SiC—Si 3 N 4 composite material manufactured according to an embodiment of the present invention. when the N source/C source ratio is 0.4 to 2, the content ratio of Si 3 N 4 is about 10% to 70%, including a certain content ratio in the SiC—Si 3 N 4 composite material; It was confirmed that excellent thermal shock strength can be secured.

図５は、本発明の一実施形態により製造されたＳｉＣ－Ｓｉ３Ｎ４複合材料のＮソース／Ｃソース比＝２によるＳｉ３Ｎ４の含量比が６９％であれば、２－ｔｈｅｔａによる強度値グラフであり、β－ＳｉＣとα－Ｓｉ３Ｎ４結晶構造を意味し、Ｓｉ３Ｎ４の含量比により各 結晶構造のメインピークの回折強度比が変わる。図５に示すように、Ｓｉ３Ｎ４の含量比が６９％であれば、Ｓｉ３Ｎ４のメインピーク回折強度／ＳｉＣメインピークの回折強度比が１．５になる。 FIG. 5 shows the SiC-Si 3 N 4 composite material manufactured according to one embodiment of the present invention, where the N source/C source ratio = 2 and the Si 3 N 4 content ratio is 69%, according to 2-theta It is an intensity value graph, which means β-SiC and α-Si 3 N 4 crystal structures, and the diffraction intensity ratio of the main peak of each crystal structure changes according to the content ratio of Si 3 N 4 . As shown in FIG. 5, when the Si 3 N 4 content ratio is 69%, the ratio of Si 3 N 4 main peak diffraction intensity/SiC main peak diffraction intensity ratio is 1.5.

図６は、実施形態により製造されたＳｉＣ－Ｓｉ３Ｎ４複合材料のＳｉ３Ｎ４含量による熱衝撃強度の変化を示したグラフであり、Ｓｉ３Ｎ４の含量が４０％を超過する時点で熱衝撃強度が６００℃以上であり、Ｓｉ３Ｎ４の含量が８０％未満になるときまで、熱衝撃強度が７００℃未満まで急速に増加することが確認される。 FIG. 6 is a graph showing changes in thermal shock strength according to the Si 3 N 4 content of the SiC-Si 3 N 4 composite material manufactured according to the embodiment, when the Si 3 N 4 content exceeds 40%. It is confirmed that the thermal shock strength is above 600° C. and increases rapidly to less than 700° C. until the content of Si 3 N 4 is less than 80%.

上述したように実施形態がたとえ限定された実施形態と図面によって説明されたが、当技術分野で通常の知識を有する者であれば前記の基材から様々な修正及び変形が可能である。例えば、説明された技術が説明された方法と異なる順序で実行される、及び／又は説明された構成要素が説明された方法と異なる形態で結合又は組み合せわされる、他の構成要素又は均等物によって代替、置換されても適切な結果が達成されてもよい。従って、他の実現、他の実施形態及び特許請求の範囲と均等のものなども後述する特許請求の範囲の範囲に属する。 Although the embodiments have been described by way of even limited embodiments and drawings as described above, various modifications and variations can be made from the foregoing substrates by those of ordinary skill in the art. For example, other components or equivalents in which the described techniques are performed in a different order than in the manner described and/or the components described are combined or combined differently than in the manner described. may be substituted and achieved with suitable results. Accordingly, other implementations, other embodiments, and equivalents of the claims are within the scope of the following claims.

Claims (7)

鋳型を準備するステップと、
前記鋳型上に１１００℃～１６００℃で、Ｓｉ、Ｎ、及びＣを含む原料ガスを導入してＳｉＣ－Ｓｉ３Ｎ４複合材料を形成するステップと、
を含み、
前記ＳｉＣ－Ｓｉ３Ｎ４複合材料のうちＳｉ３Ｎ４は、４０体積％～７０体積％であり、前記ＳｉＣ－Ｓｉ ３ Ｎ ４ 複合材料を形成するステップはＣＶＤ法に基づく、ＳｉＣ－Ｓｉ３Ｎ４複合材料の製造方法。 preparing a mold;
introducing a raw material gas containing Si, N, and C onto the mold at 1100° C. to 1600° C. to form a SiC—Si 3 N 4 composite material;
including
Si3N4 in the SiC- Si3N4 composite material is 40% by volume to 70% by volume , and the step of forming the SiC- Si3N4 composite material is based on a CVD method , SiC-Si A method for making 3N4 composites. 前記導入する原料ガスのうち、窒素（Ｎ）と炭素（Ｃ）原料ガスの窒素（Ｎ）成分と炭素（Ｃ）成分が１：１である場合、Ｎソース／Ｃソースの体積比率が０．４～２である、請求項１に記載のＳｉＣ－Ｓｉ３Ｎ４複合材料の製造方法。 When the nitrogen (N) component and the carbon (C) component of the nitrogen (N) and carbon (C) source gases of the introduced source gas are 1:1, the volume ratio of the N source/C source is 0.1. 4 to 2, the method for producing a SiC-Si 3 N 4 composite material according to claim 1. 前記ＳｉＣ－Ｓｉ３Ｎ４複合材料の熱衝撃強度は、５００℃～８６０℃である、請求項１に記載のＳｉＣ－Ｓｉ３Ｎ４複合材料の製造方法。 The method for producing a SiC-Si 3 N 4 composite material according to claim 1, wherein the SiC-Si 3 N 4 composite material has a thermal shock strength of 500°C to 860°C. 前記ＳｉＣ－Ｓｉ３Ｎ４複合材料の熱衝撃強度は、６００℃～８６０℃である、請求項１に記載のＳｉＣ－Ｓｉ３Ｎ４複合材料の製造方法。 The method for producing a SiC-Si 3 N 4 composite material according to claim 1, wherein the SiC-Si 3 N 4 composite material has a thermal shock strength of 600°C to 860°C. ＳｉＣ及びＳｉ３Ｎ４を含み、熱衝撃強度が６００℃～８６０℃であるＳｉＣ－Ｓｉ３Ｎ４複合材料であって、
前記ＳｉＣ－Ｓｉ３Ｎ４複合材料のうち前記Ｓｉ３Ｎ４は、４０体積％～７０体積％であり、前記ＳｉＣ－Ｓｉ ３ Ｎ ４ 複合材料はＣＶＤ法に基づいて形成される、ＳｉＣ－Ｓｉ３Ｎ４複合材料。 A SiC—Si 3 N 4 composite material comprising SiC and Si 3 N 4 and having a thermal shock strength of 600° C. to 860° C.,
The Si3N4 content of the SiC- Si3N4 composite material is 40% by volume to 70% by volume , and the SiC-Si3N4 composite material is formed based on a CVD method . Si3N4 composites . 前記ＳｉＣ－Ｓｉ３Ｎ４複合材料は、不定形のＳｉＣ結晶粒と針状構造のＳｉ３Ｎ４結晶粒が混合されている、請求項５に記載のＳｉＣ－Ｓｉ３Ｎ４複合材料。 The SiC-Si 3 N 4 composite material according to claim 5 , wherein said SiC-Si 3 N 4 composite material is a mixture of amorphous SiC crystal grains and acicular Si 3 N 4 crystal grains. 前記ＳｉＣ－Ｓｉ３Ｎ４複合材料のうち、前記Ｓｉ３Ｎ４の体積比が６８体積％～７０体積％である場合、Ｓｉ３Ｎ４／ＳｉＣメインピークの回折強度比は０．２～１．５である、請求項５に記載のＳｉＣ－Ｓｉ３Ｎ４複合材料。 When the volume ratio of Si3N4 in the SiC- Si3N4 composite material is 68% to 70% by volume, the diffraction intensity ratio of the Si3N4 /SiC main peak is 0.2 to 1 . The SiC-Si 3 N 4 composite according to claim 5 , wherein .5.
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